Production process of oxytetracycline dihydrate hydrochloride
A technology of oxytetracycline hydrochloride and production process, which is applied in the field of production process of large particle oxytetracycline hydrochloride, can solve the problems of low yield and low apparent density, achieve high apparent density, meet different requirements, and have good fluidity
Inactive Publication Date: 2009-11-04
大丰华曙药业有限公司
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[0005] The object of the present invention is to overcome the defects of low apparent density or low yield of the products produced by the above four large particle oxytetracycline hydrochloride production processes, and provide a new large particle oxytetracycline hydrochloride production process
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[0008] Add isopropanol-n-butanol to the reaction kettle, control the temperature at 15-20°C, add hydrogen chloride-n-butanol, control the temperature at 22-28°C, add oxytetracycline under stirring until clear, add activated carbon and stir Decolorize for 5 minutes, press filter to obtain the solution, raise the temperature of the solution to 45-50°C and keep it warm for 1.5-2 hours, cool down to below 30°C, filter and wash with n-butanol, and vacuum-dry the crystal at below 90°C for 4 hours.
[0009]
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The invention relates to a production process of oxytetracycline dihydrate hydrochloride, in particular to a process for preparing oxytetracycline dihydrate hydrochloride by the steps of salifying and crystallizing through using oxytetracycline as the raw material and isopropanol-normal butanol as crystallized solvent and adding chlorine hydride-normal butanol. Four production processes of oxytetracycline dihydrate hydrochloride are provided both here and abroad, and oxytetracycline hydrochloride obtained by the four prior production processes has low apparent density and poor fluidity either, or low yield and high cost. The oxytetracycline hydrochloride obtained by the production process of oxytetracycline dihydrate hydrochloride, which is provided by the invention, has high apparent density, good fluidity and high yield.
Description
technical field [0001] The production process of large particle oxytetracycline hydrochloride belongs to the field of biomedicine. Oxytetracycline hydrochloride is a broad-spectrum antibiotic drug, which is widely used for infections of various Gram-positive cocci and Gram-negative bacilli, and is also used for macule Typhoid fever, scrub typhus and Rickettsia infection and certain virus infection. Background technique [0002] There are 4 kinds of large particle oxytetracycline hydrochloride production processes at home and abroad, all of which use oxytetracycline as raw material and use different crystallization solvents. [0003] The first production process uses methanol + acetonitrile as the crystallization solvent; the second uses methanol + ethyl acetate as the crystallization solvent; the third uses methanol + isopropanol as the crystallization solvent; the fourth uses n-butanol as the crystallization solvent. [0004] The products formed by the first three syntheti...
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IPC IPC(8): C07C237/26C07C231/12C07C231/22A61P31/04
Inventor 陈天生蔡紫阳
Owner 大丰华曙药业有限公司
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